CN1114566C - Methods for treating semiconductor wafers - Google Patents

Methods for treating semiconductor wafers Download PDF

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Publication number
CN1114566C
CN1114566C CN98805967A CN98805967A CN1114566C CN 1114566 C CN1114566 C CN 1114566C CN 98805967 A CN98805967 A CN 98805967A CN 98805967 A CN98805967 A CN 98805967A CN 1114566 C CN1114566 C CN 1114566C
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solution
bhf
electronic component
ammonium hydroxide
source
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CN1259925A (en
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史蒂文·维哈费尔贝克
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CFMT Inc
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CFMT Inc
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H01L21/02052—Wet cleaning only
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075—Cleaning of glass
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/06—Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/10—Salts
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
    • H01L21/02008—Multistep processes
    • H01L21/0201—Specific process step
    • H01L21/02019—Chemical etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31105—Etching inorganic layers
    • H01L21/31111—Etching inorganic layers by chemical means
    • C11D2111/22—

Abstract

The present invention presents methods for, inter alia, cleaning and etching semiconductor wafers with a solution containing ammonium fluoride and control of the process used for preparing such a solution at its point of use.

Description

The method of process semiconductor wafers
Invention field
Solution-treated (corrosion and/or the cleaning) semiconductor wafer that the present invention relates to the fluorinated ammonium reaches the technology controlling and process field of using this solution of some preparation at it.
Background of invention
Can adopt different solutions to clean and corrode semiconductor wafer.Recently, general cleaning solution has been prepared in particular for the solution of oxide etch design contained Neutral ammonium fluoride is wherein cleaned or corrodes compound as main.In this case, the semiconductor processes unit is designed to deposit the ammonium fluoride solution that has prepared, uses these solution then when semiconductor processes person needs.
This solution is called buffered HF solution, is by the salt Neutral ammonium fluoride (NH as faintly acid hydrofluoric acid and this acid 4F) mixture constitutes.Originally the development of this mixture is become the rare HF of buffering, thereby (be several days to several weeks) obtains the constant erosion rate in the time cycle that prolongs.This solution is called as buffered HF (BHF), and term BOE (buffered oxide etch) also is used to represent this solution.Therefore, suitable solution (being BHF or dHF) be can select, the particular etch and/or the cleaning step that will carry out optimized.
Yet, find that the character of buffered hydrofluoric acid and rare HF is slightly different, except that shock absorption, also favourable to semiconductor processing device under several situations.
The main difference of BHF and dHF is that the pH value of solution is different.The pH value of BHF is about 3-5, and the pH value of dHF is about 1-2.So, the active substance difference in the solution.
Owing to following reason, adopt BHF that prospect is arranged very much in some semiconductor processes is used: (1) is because the higher pH value of BHF, so for BHF corrosion stability comparison dHF (rare HF) more " stablize " (2) BHF have be different from dHF the corrosion selection rate (for example, when BPSG (boron-phosphorosilicate glass) is lower than the selection rate that obtains with respect to the thermal oxide selection rate, adopt BHF in dHF; If or proportioning is suitable, BHF also can obtain opposite result (that is, it can provide the erosion rate higher than thermal oxide for BPSG); (3) under identical fluoride concn, BHF can provide the oxide etch speed higher than dHF; (4) BHF can also provide higher nitride etch speed; (5) it is different with dHF that BHF stops the surface; And (6) in some cases, and the higher pH value of BHF can provide improved particle performance according to the special role of zeta-potential.
The BHF technology is pre-mixed solution routinely, is used for the wet processing unit then.Adopt pre-mixing BHF that several problems are arranged.For example, particulate becomes problem; This particle can damage the integrated level of the finished product.Because the high viscosity of BHF and surface tension, high erosion rate and under wet bench (wet bench) situation, wafer are put into treatment trough or the continuation corrosion when treatment trough takes out and enter rinse tank, have all limited the corrosion homogeneity.In addition, because pre-mixing BHF generally is used for time expand,,, endanger the integrated level of the finished product once more so metallic impurity may be introduced treatment solution sometimes up to a week.In addition, BHF is tending towards crystallization being lower than under 16-17 ℃ the temperature, has produced the pre-mixing chemical reagent carries out the commercial transportation aspect from different local (that is the suppliers of water treatment plant) problem.Because pre-mixing BHF has high viscosity and surface tension, thus generally need tensio-active agent to improve its wettability, and reduce particulate formation.At last, use pre-mixing BHF, NH 4The premix ratio of F and HF is limited in 6: 1,7: 1 or 10: 1, limited the handiness of handling.Adopt pre-mixing BHF also expensive in addition.
Although it is quite useful to utilize BHF to handle the electronic component predecessor, need to reduce the problem relevant with pre-mixing BHF.The present invention is devoted to overcome these problems and satisfies other requirement.
Summary of the invention
The invention provides and improve cleaning or corrode the particularly method of oxide etch semiconductor wafer of semiconductor wafer, adopt fluorinated ammonium (NH 4F), and better be the cleaning/corrosive water solution that also contains hydrogen fluoride (HF) or (hydrofluoric acid).This solution may also be referred to as buffered HF solution (BHF) or buffered oxide etch (BOE) solution.Method of the present invention is used for using in the semiconductor processes district place of this solution directly to prepare this BHF solution, or hydrofluoric acid is mixed to come " preparation " with alkali, or comes " preparation " in the processing vessel by they are injected into.Available hydrogen fluoric acid and ammonium hydroxide are prepared this solution.In this way, the present invention is useful to the semi-conductor processor.An advantage is, because starting material reagent--hydrogen fluoride (hydrofluoric acid) aqueous solution and ammonium hydroxide aqueous solution have been used for other treatment step, just can introduce method of the present invention in its operating process so need not that semiconductor processing device is carried out significant improvement; So the present invention can make the processor not use overall chemical reagent (pre-mixing BHF) in treatment zone.Another advantage is that the inventive method can reduce problem relevant with particle in the treatment system.In addition, the present invention can provide the corrosion homogeneity than conventional BHF technology excellence.An advantage is again, and the present invention can improve the purity of BHF solution, and reduces concentration of metallic impurities.At last, the present invention can improve the processing handiness using point that any ratio of mixture is provided.This ratio of mixture changes easily by any way.
Utilize to use the point of BHF solution, can observe 0.16 micron granule number be generally negative, for example-100 to-200.In addition, utilize the point that uses BHF, even do not use the corrosion homogeneity is optimized, also obtain the corrosion homogeneity of 2-3% easily.Utilize the point that uses BHF,, also be reduced to minimum even pollution relevant with metallic impurity and crystallisation problems are not eliminated.Designed BHF does not generally need tensio-active agent, and the NH of any ratio of mixture can also be provided 4F and HF owing to can provide additional handiness to the wet processing technology, for given semiconductor processes, can make erosion rate and selection rate the best, so be useful.Designed BHF also has the higher ratio of performance to price, the reasons are as follows: (1) is because each chemical reagent generally is used for other wet processing step, so do not need extra chemical reagent pipeline in the decontamination chamber; (2) because each chemical reagent generally is used for other wet processing step, so also do not need chemical reagent is limited and quality control; (3) do not need the Surfactant Chemistry waste treatment.
In one embodiment of the invention, the method with the solution-treated semiconductor wafer of fluorinated ammonium may further comprise the steps.At first, provide ammonium hydroxide (NH 4OH) source and hydrogen fluoride (HF) source.Then, ammonium hydroxide is directly delivered in the processing vessel from the ammonium hydroxide source, and hydrogen fluoride is directly sent into processing vessel from the hydrogen fluoride source, preparation comprises Neutral ammonium fluoride (NH 4F) and the treatment soln of HF.A plurality of semiconductor wafers are contacted with treatment solution, remove the useless material on the semiconductor wafer.
In the gained treatment solution, NH 4The volumetric molar concentration of F is preferably about 0.02 to about 20, and the volumetric molar concentration of HF is preferably about 0.01 to about 30.NH 4F is preferably the 0.01-10 mol, and HF is preferably the 0.10-20 mol.
Treatment solution can be used for various situations, when for example having oxide compound, nitride, titanium (being not limited to these), is used to corrode the surface of semiconductor wafer or the general cleaning of semiconductor wafer.
Brief description
Fig. 1 represents the relation between erosion rate and fluoride concn.
Fig. 2 represents that total fluoride concn is that 2 mol are (corresponding to H 2O: the HF thinning ratio is 14: 1) time, the relation of relative concentration of different substances in the BHF solution (total fluoride concn ratio) and pH value.
When Fig. 3 represents that total fluoride concn is 0.14 mol, the relation of the relative concentration of different substances and pH value in the BHF solution.
Fig. 4 represents [HF 2 -]/[HF] than and H 2Relation between the thinning ratio of O: HF.
Fig. 5 represent CFM technology company 8100 full stream (Full-flow) system, a kind of example that can be used for implementing wet treatment system of the present invention.
Fig. 6 represents unitary container area shown in Figure 5, has showed the slit of placing the electronic component predecessor during handling.
Fig. 7 represents to be fixed in the full stream of CFM technology company TMWafer in the container of system.
The detailed introduction of invention
Terminology used here " active treatment fluid ", " activity chemistry treatment fluid ", " treatment fluid ", " chemical liquids ", " active chemical agent ", " activity chemistry treatment fluid " or " treatment fluid ", refer to during manufacture, the electronic component predecessor is exposed to wherein, and the active liquid of certain effect occurs in effects on surface electronic component predecessor, to be different from such as rinsing liquid such as DI water. These terms can exchange. With term " treatment fluid ", " active (reactive) " or " active (active) " when being combined with, refer to for example particle, metal impurities or organic matter in the removal electronic component predecessor are had the treatment fluid of certain effect, or refer to that there is the treatment fluid of certain effect on surface to etching electronic element predecessor, or refer to the effective treatment fluid of oxide layer of growing on electronic component predecessor's surface, but be not limited to these. The example of this activity chemistry treatment fluid is that concentration can be greater than 1000: 1 (H2O: hydrofluoric acid HF) (HF) aqueous solution.
Terminology used here " nonactive chemical treatment fluid " refers to the treatment fluid that for example needn't work to the contamination of removing in the electronic component predecessor can comprise rinsing liquid.
Here used term " chemical treatment step " refers to the electronic component predecessor is exposed in a kind of activity chemistry treatment fluid.
Here used term " processing " refers to some active step that the electronic component predecessor is carried out, for example cleans or corrosion.
Here used term " wet type processing " refers to the electronic component predecessor is exposed in a kind of or a series for the treatment of fluid, thereby for example cleans or etching electronic element predecessor's surface.
Here used term " rinsing liquid (rinsing liquid) " or " rinsing liquid (rinse liquid) " are meant that DI water or some are used for other liquid of rinsing electronic component predecessor after being exposed to the activity chemistry treatment solution, as with the comparison of chemical reagent.Rinsing liquid can be a DI water, or very rare chemical reagent aqueous solution (for example hydrochloric acid), to prevent the lip-deep metal deposition of electronic component predecessor (adopting very rare hydrochloric acid soln) during for example rinsing.Ozone is another additive that adopts during the rinsing.Chemical concentrations in this rinsing liquid is very low, and generally its concentration is not more than about 100ppm.The main effect of rinsing liquid is to remove lip-deep chemical reagent of electronic component predecessor or reaction product, rather than certain " activity " is carried out on electronic component predecessor's surface handle.
Here used term " reaction chamber " is meant that container, full fluid capacitance device or monophyly, groove, wet bench and other are applicable to the container of wet processed method.This term and term " processing vessel " can exchange.
Terminology used here " full fluid capacitance device " is meant the container with respect to environmental sealing, generally is used for " Quan Liufa ", or is sometimes referred to as single tank systems.
Here used term " electronic component predecessor (precursor) " comprises semiconductor wafer, flat board and is used for electronic component (that is, unicircuit) other parts in making, but is not limited to these.
Method of the present invention generally can be applicable to any wet processed equipment.Be suitable for implementing reaction chamber of the present invention and comprise full fluid capacitance device, single-process-chamber, wet bench (groove) and jet cleaning system etc., but be not limited to these.For example, (Werner Kern edits referring to semiconductor wafer cleaning technique handbook, Noyes Publication Parkridge publishes, 1993, New Jersey) chapter 1 in: overview and the development (Werner Kern) and the chapter 3 of semiconductor wafer contamination and cleaning technique: aqueous solution clean (Don C.Burkmak, Donald Deal, Donakd C.Grant and Charlie A Peterson), (Tadahiro Ohmi edits to reach the ultra clean technology handbook, the MarcelDekker publication) in the first roll, the wet corrosion of being write by Hiroyuki Horiki and Takao Nakazawa cleans, and integral body is quoted these documents here.Specific preferred wet treatment system is that 8100 of CFM technology company flows entirely TMSystem.
For example, people's such as P.Gise semi-conductor and ic manufacturing technology (RestonPublishing Co.Reston, Va.1979) in generality introduced semiconductor fabrication, integral body is quoted the document here.
Be suitable for implementing activity chemistry treatment solution of the present invention and comprise hydrochloric acid and damping fluid thereof (promptly, the damping fluid that contains hydrochloric acid), mixture, hydrofluoric acid and damping fluid thereof, chromic acid and damping fluid thereof, phosphoric acid and damping fluid thereof, acetate and damping fluid thereof, nitric acid and damping fluid thereof, Neutral ammonium fluoride and damping fluid thereof, ammonium hydroxide and damping fluid thereof and the aqueous solution of hydrofluoric acid and damping fluid thereof and their combination of ammonium hydroxide and damping fluid, hydrogen peroxide and damping fluid thereof, sulfuric acid and damping fluid thereof, sulfuric acid and ozone, but be not limited to these.No matter when, BHF can be used for the wet processed technology.Used special processing liquid, equipment used, exposure duration and experiment condition (that is, temperature, concentration and treatment solution flow) will change according to the specific purpose of wet processed method.
The activity chemistry treatment solution can also comprise additional additive, for example, and tensio-active agent, complexing or sequestrant and inhibiter.
Be suitable for implementing nonactive chemical treatment solution of the present invention and comprise deionized water or the very rare deionized water and/or the solution of chemical reagent, but be not limited to these.The example of this reagent has hydrochloric acid, hydrofluoric acid, nitric acid, hydrogen peroxide, ozone and tensio-active agent, but is not limited to these.
After the chemical treatment, available well-known to one skilled in the art any method makes electronic component predecessor drying.
The inventive method can be used for corroding or cleaning the surface of semiconductor wafer, thereby removes layer or its part that silicon face is taken up an official post and why not wanted, for example zone of oxidation, nitride layer, aluminium lamination, titanium layer (being not limited to these layers).The present invention also can be used for the controlled oxide corrosion.
The invention provides the salt Neutral ammonium fluoride (NH that is used to contain as faintly acid hydrogen fluoride and this acid 4The method of buffered hydrogen fluoride F) (BHF) aqueous solution.This BHF solution is used for cleaning or corrosion electronic component predecessor, for example semiconductor wafer, flat board, and other electronic component predecessor.Below will introduce the present invention at cleaning or corroding as the semiconductor wafer of electronic component predecessor representative.Cleaning or the corrosion step implemented by this BHF solution can comprise that general wafer cleans, and is specially adapted to the oxide etch of wafer.Yet, the invention is not restricted to this purging method.
According to the present invention, directly prepare BHF solution in its final place of using.BHF can be in tempering tank by its each component preparation, be sent to then and mix the processing vessel that the tank liquor road is connected, or in processing vessel itself, make and prepare BHF.In this way, can in the treatment chamber of semiconductor processor, prepare BHF solution with the various chemical reagent that generally are used for other processing of this wafer.This can make the amount minimum that need be stored in the former chemical reagent among treatment zone or " manufacturing district (fab) ", thereby has simplified treatment zone.
The exemplary process district of process semiconductor wafers will have for example ammonium hydroxide (NH 4OH) and the storage tank of hydrofluoric acid chemical reagent such as (HF).These reagent are generally stored with the strong solution form.For NH 4OH, strong solution is generally the aqueous solution of about 29wt%, and for HF, strong solution is generally the aqueous solution of about 49wt%.These solution also can be preserved NH with the form of dilution 4The minimum concentration of OH solution is that about 400 parts of water are than 1 part of NH 4OH, HF solution has identical minimum concentration.
The method according to this invention, BHF treatment solution directly are prepared in the place of its application in the treatment zone, are used for cleaning and/or the corrosion semiconductor wafer.In one embodiment, in processing vessel, make the BHF treatment solution.Processing vessel and NH 4The storage tank of OH and HF solution has the liquid road to be connected.Can use control valve and control pump as the treatment facility between these storage tanks and processing vessel.In this way, for example process control system such as PC can be used as control and monitors every kind of solution NH 4Thereby OH and the HF solution interpolation speed in processing vessel prepares the device of this treatment solution.
By with a selected amount of NH 4The OH aqueous solution and a selected amount of HF aqueous solution prepare the BHF treatment solution together.These two kinds of compound reactions form NH 4F.Thereby these two kinds of reactive material contain NH by the excessive formation of the mole number that makes HF 4The ratio combination of the final BHF treatment solution of F and HF.Preferably contain volumetric molar concentration in the BHF treatment solution and be about 0.02 to about 20 NH 4F (solution of mol).Also contain about 0.01 to 30 the HF of volumetric molar concentration.NH 4F is preferably the 0.10-10 mol, and HF is preferably the 0.10-20 mol.The BHF treatment solution also can be excessive HF preparation, thereby in the BHF treatment solution, be difficult for measuring HF, although there is excessive HF to exist for.
At NH 4OH solution and HF solution are sent in the processing vessel, form the BHF treatment soln after, for example any pump of equipment and/or the valve that are used to transmit these reagent can be closed.The BHF treatment soln to be to form in its final some form to be used of using, and cleans and/or corrodes silicon wafer.This step can utilize various known contact procedures to finish.A kind of such method is that wafer is immersed in the BHF treatment solution in the processing vessel.Other method is to make BHF liquid flow through wafer or treatment solution is ejected on the wafer.
The temperature of BHF treatment solution can be maintained at about 3 ℃ to about 90 ℃, better is about 15 ℃ to 70 ℃, is preferably in 20-40 ℃.
Mix independent NH 4OH and HF solution form the technology of BHF treatment solution and can carry out automatically to a certain extent.That is, the concentration known of these solution can be imported in the computer, controls the interpolation speed of every kind of solution then with a program, forms desired NH in the final BHF treatment solution 4F and HF concentration.
BHF treatment solution of the present invention is preferred for the oxide etch treatment step, so that remove the silicon oxide on the semiconductor wafer surface.Undesired oxide compound comprises PBSG oxide compound and thermal oxide.
According to the present invention, it uses some preparation BHF treatment solution in treatment zone, stores NH in treatment zone 4F and directly solution is sent to and is used as the treatment solution aspect in the processing vessel has many places that are better than prior art that have.For example, adopt method of the present invention, can significantly reduce particulate accumulation in the treatment system.In addition, method of the present invention can be improved the homogeneity of etching process.According to the present invention, HF and NH 4Between the OH solution any ratio of mixture can be arranged.In addition, owing to can save the independent NH of processing 4Needed space of F solution and equipment, thus work simplification of the present invention treatment zone,
Without departing from the spirit of the invention, can be by hydrofluoric acid and alkali, mix with ammonium hydroxide as preferred bases, using some preparation BHF solution.Be suitable for implementing other alkali of the present invention and comprise Tetramethylammonium hydroxide, but be not limited thereto.
Following example is used for explaining, and unrestricted the present invention.Examples Example 1
Experiment determines to inject altogether BHF speed and selectivity
1 experimental design
In first experimentalists and technicians that constitute by 23 corrosion experiments, adopt thermal oxide and silicon nitride wafer, scanning mixes NH 4The whole dynamicrange of OH and HF.The HF that changes blended or inject altogether is so that for every kind of NH 4(ratio just forms NH to the excessive HF of OH combined amount (or injection rate) 4The HF that the needed amount of F is many) 10% to 100%.
At second experimentalists and technicians, from these 23 previous experiments, select 8 corrosion experiments, the BHF corrosion selectivity of research thermal oxide corrosion and BPSG and TEOS oxide compound.
Erosion rate and selectivity experiment are flowed entirely in CFM technology company 8100 TMCarry out in the system.
2 dynamicranges
Flow entirely in 8100 of CFM technology company TMInject NH in the system 4The dynamicrange of OH is 400: 1 to 3: 1.When having excessive HF, the NH of each mole 4OH will react with HF, form the NH of a mole 4Therefore F, flows entirely in 8100 of CFM technology company TMIn the system, NH 4The dynamicrange of F is that 0.0426 mol is to 5.686 mol.If provide NH with 40%-w solution 4F, then this will be corresponding to H 2O: NH 4254: 1 and 1.89: 1 the thinning ratio of F (40%-w).In other words, the dynamicrange of the full stream of CFM is corresponding to the NH of 0.15%-w21%-w 4F or NH 4OH concentration.
Study this dynamicrange, simultaneously with excessive HF concentration from NH 410% of F concentration is adjusted to 100%, and (excessive HF is from NH 410% of F volumetric molar concentration changes to 100%).
3 experiments
The design of a experiment condition
Table 1 shows the experimental design of first serial experiment.In this table, show injection with respect to HF than (that is H, 2O: NH 4OH: HF).NH 4F has covered CFM8100 and has flowed entirely TM(400: 1-10: in the whole dynamicrange 1).[HF]/[NH 4F] ratio between 10% to 100%, change.
In second group of experiment, select 8 corrosion experiments, carry out with different oxide compounds.In each experiment, with 5 wafers: 1 one is the thermal oxide wafer in order to be used for the additional natural oxide wafer of testing of particle, and one is the BPSG wafer, and one is the TEOS wafer, and one is the silicon nitride wafer.Back four wafers are corroded homogeneity and selectivity test.
4 results
CFM flows entirely TMThe prescription of BHF seems and SCl (H in 8100 2O 2, NH 4OH, and H 2O) or SC2 (H 2O 2, HCl and H 2O) step is similar.This step is called HF/NH 4OH.Can be used for CFM8100 flows entirely TMThe example of one group reaction condition of system experimentation is as follows: flow condition 20gpm; 35 ℃ of temperature condition; 60.0 seconds soak times of injection length 60.0 seconds; The ratio 100 of water; The ratio 0.77NH of HF 4The ratio 1 of OH; Mega sonic wave ON 0.0 second; Mega sonic wave OFF 0.0 second
A converts
NH from prescription 4OH and HF and H 2The volume ratio of O, can calculate and the following:
If prescription input (volume ratio)
H 2O＝a NH 4OH＝b HF＝c
Then [HF] concentration of injecting by mol is HF
＝c/a*1000*1.18*(49/100)/20.006*(a/(a+b-1-c))
In this formula, the specific density of supposing HF in the solution of 49%-w is 1.18, and HF is provided in the injection tube by the concentration in HF weight 49%.In addition, the molecule of supposing HF heavily is the 20.006g/ mole.Can followingly determine [NH 4OH]
[NH by the mol injection 4OH]=b/a *0.9 *(29/100) *1000/17 *A/ (a+b+c).
In this formula, suppose NH in 29% solution 4The specific density of OH is 0.9, and with NH 4OH presses with NH 3The concentration of weight meter 29% is provided in the injection tube.In addition, suppose NH 3Molecule heavily be the 17g/ mole.
B discusses and further converts
The HF and the NH that inject 4OH will form HF and NH 4F.Specifically, this HF and NH 4F will form HF, HF 2 -, F -, NH 4With the more high polymers of HF for example (HF) 2Directly inject HF and NH by injection tube 4F can produce the material of same concentrations in container.Can calculate HF and NH 4F be injected in the pipeline so that in the container each active substance reach the needed amount of equivalent concentration (prerequisite be really to have injected HF and NH 4After the OH).Suppose and injected normal [HF] and [NH 4F] (if inject HF and NH 4F replaces HF and NH 4OH):
NH 4[NH in the F-HF scheme 4F]=NH 4[NH in the OH-HF scheme 4OH]
NH 4[HF]=NH in the F-HF scheme 4[HF]-[NH in the OH-HF scheme 4OH]
Therefore, [HF]/[NH 4F] ratio be
[HF]/[NH 4F]＝([HF]-[NH 4OH])
CHF/NH 4The conversion of F is (with respect to NH 4The mole of OH/HF (volume))
For with [HF]/[NH 4F] than converting NH to 4The volume ratio of OH (29%)/HF (49%) can be used following chemical formula: as [HF]/[NH 4F]=0 o'clock
NH 4OH(29％)/HF(48.9％)＝1.8825/([HF/[NH 4F]+1)，
Thereby NH 4OH/HF=1.8825
Therefore, NH 4OH is 1.8825 with the maximum volume ratio that HF injects.
5 measure
On a wafer
On oxide wafer, nitride wafers and testing wafer (natural oxide), the oxide compound that is corroded (25 points do not comprise the 6mm edge), the nitride (25 points do not comprise the 6mm edge) that is corroded, particle removal (＞0.16 micron does not comprise the 5mm edge).Utilize the Tencor Surfscan 6220 of CFM Apps Lab. to measure particle.Utilize Flanders, the Rudolph FE VII-D of Rudolph Technologies measures thickness among the NJ..
On the b equipment
Actual volume (with respect to the proportioning volume), temperature, the electric conductivity of the DI stream when injecting end, the chemical reagent that injects.Carry out each experiment with three wafers.A nitride wafers places slit #22, and the thermal oxide wafer places slit #32, and testing wafer places slit #42 (slit as shown in Figure 7).
6 first and second groups of result of experiment
Because by mixing NH 4OH and HF prepare NH 4F is so data can be expressed as NH 4The function of OH and HF is as doing in the table 1.Provide the thinning ratio of HF on the Z-axis, provided NH on another axle with respect to water 4The ratio of OH and HF.NH 4The ratio of OH and HF is 1.8825 to have drawn good NH 4F solution (promptly not having excessive HF).Higher ratio will form NH 4OH and NH 4F rather than HF and NH 4F.
Table 1. is with dust/minute be unit, thermal oxide erosion rate in the time of 40 ℃.Some experiment is carried out at 35 ℃.35 ℃ of experiments of carrying out are with less character representation.Data are expressed as NH 4The function of OH and HF.Provided NH 4OH and H 2O is with respect to the volume ratio of 1 part of HF.So volume ratio is expressed as H 2O: NH 4OH: 1, wherein 1 is HF.0NH 4The data of OH are standard C FM data of rare HF solution.
NH 3 H 2O∶HF 0 0.85 0.70 0.73 0.74 0.75 0.76 0.78 0.81 0.84 0.97 0.99 1.1 1.5 1.7 1.8 1.88 2.0 2.1 2.4
500∶1 10
400∶1 7
357∶1
333∶1
294∶1 18
270∶1 14
250∶1 16
232∶1 17
204∶1 20
200∶1 25
189∶1 ?26 ?27
182∶1
175∶1 32 32
154∶1
150∶1 33
147∶1 ?35C/21
127∶1 35C/36
125∶1 40
116∶1 35C/21
111∶1 48 35C/46
101∶1 19
100∶1 50
98∶1
92∶1 68
90∶1 5
89∶1
88∶1
85∶1
80∶1 82
74∶1
70∶1 71
68∶1
65∶1
63∶1 ?156
60∶1 83
53∶1
50∶1 99 2 (corrosion silicon)
48∶1 129 (corrosion silicon)
40∶1 123 ?83
37∶1 ?411(？) 247 3 (corrosion silicon)
35∶1 140
29∶1 he) 3 (corrosion silicon)
23∶1 ?263 ?37 3 (corrosion silicon)
16∶1 ?＞840 ＞353 ?404
13∶1 ＞528
11∶1
At H.Kikuyama, N/Miki, K.Saka, J.Takano, I.Kawanabe, people such as M.Miyashita and T.OHmi are published in the 4th the 1st phase of volume of IEEE Trans On Semic.Manuf. (the IEEE semi-conductor is made transactions), in the article of 26 pages (1991), reported the HF and the NH of reciprocity mol ratio 4F obtains the situation of high erosion rate.About NH 4The volume ratio of OH and HF, this is corresponding to NH 4The volume ratio of OH/HF=0.94.
If with ratio be 1: 0.86 to 1: 1.2 NH 4OH is plotted on the curve with respect to the HF thinning ratio with the corrosion data of the mixing solutions of the HF corrosion data with rare HF, and Fig. 1 is its result.Fig. 1 has showed [NH 4OH] concerning the influence of erosion rate for more and more important 100: 1 and the lower thinning ratio.The dHF solution identical with HF concentration is compared, and is 100: 1 o'clock in thinning ratio, and the erosion rate among the BHF is high approximately by 20%, is 70: 1 o'clock in thinning ratio, and the erosion rate among the BHF is fast approximately 50%, is 63: 1 o'clock in thinning ratio, the erosion rate among the BHF fast approximately 100%.It seems that thinning ratio is higher than 100: 1, erosion rate does not depend on NH very much 4The concentration of OH.These results conform to theory very much.
In BHF, there is following material: H +, OH -, F -, HF 2 -, HF and (HF) 2In rare HF, main etching reagent is the HF molecule of disconnection and (HF) that plays the etching reagent effect 2Dipolymer.In BHF, HF 2 -Also etching of oxides.HF 2 -The speed of etching of oxides is approximately than (HF) 2And/or fast 4 times of HF.HF in the solution 2 -Existence depend primarily on the pH value of solution.
In the pH value is 3 between 5 the time, [HF 2 -] concentration ratio (HF) or (HF) 2Concentration much higher, as shown in Figure 2.Yet dramatical change takes place in this situation in dilute solution.200: 1 same curve under the solution situation have been shown, corresponding to the volumetric molar concentration of 0.14 mol among Fig. 3.In Fig. 3, be 3 to 5 o'clock in the pH value, [HF 2 -] concentration is still passed maximum value, but [HF 2 -] concentration is always far below the concentration of [HF].Can fixed pH value calculate [HF according to the function of dilute solution 2 -] with the ratio of [HF].
The pH value is 3.6 o'clock, [HF 2 -] with [HF] such as shown in Figure 4.HF 2 -Concentration only be lower than at 100: 1 o'clock and just become quite big in thinning ratio.Shown to have only thinning ratio to be lower than, NH why at 100: 1 o'clock 4The add-on of the relative HF of OH just can improve erosion rate.Even for the solution that more dilutes, NH 4OH does not change erosion rate with respect to the add-on of HF, and it will change change pH values, and this also is important for the composition corrosion, and the high more erosion to resist of pH value is more little.In addition, according to pH, have slightly different surface and stop, this is owing in the solution more F are arranged -Even F -Do not corrode SiO 2, also can interact with Si.Finally, because the different pH value of the effect of zeta-potential can cause the particle improved performance between particle and wafer surface, so NH 4The add-on of OH can influence particulate and form.Example 2
BHF and CFM technology total flow system
Because NH 4OH and HF mix will obtain NH 4So F is can be by mixing NH 4OH and HF prepare BHF.If use the HF of overrich, then obtain NH 4F and HF.Flow entirely at CFM TMIn the system, developed new software, with common injection NH 4OH and HF obtain BHF.At NH 4In the mixed solution of F and HF, general 6: 1 or 7: 1 (NH 4F: ratio HF) is prevailing, is meant NH here 4The volume ratio of F and HF, wherein NH 4F carries with 40%-w solution, and HF carries with 49%-w solution.Yet, also can use concentration in the industry up to 20: 1.NH 4The volume ratio of F: HF be 6: 1 in fact corresponding to 2.65: 1 mol ratio.At NH 4OH carries with the solution of 29%-w, and when HF carried with the solution of 49%-w, this can be 1: 1 NH by injecting volume ratio altogether roughly 4OH and HF obtain.
In fact, in 1: 1 solution, there are the HF of 24.5 mol and the NH of 17 mol 4OH.The NH of 17 mol 4The HF of OH and 17 mol will form NH together 4F, the HF of all the other 7.5 mol is excessive.This has provided mol ratio is 17: 7/5=2.3: 1 NH 4F: HF approaches 6: 1 mol ratios of 2.65: 1 in the solution.
This shows that CFM flows entirely TMIn common HF and the NH of injecting 4HF that OH is to be injected with needs and NH 4OH has similar volume, and this point is very important, because can inject two kinds of chemical reagent in processing vessel (reaction chamber) with new similar hardware.

Claims (10)

1. method with the solution-treated electronic component predecessor of fluorinated ammonium may further comprise the steps:
(a) provide ammonium hydroxide (NH 4OH) source and hydrogen fluoride (HF) source;
(b) ammonium hydroxide is directly delivered to the processing vessel from the ammonium hydroxide source, and hydrogen fluoride is directly delivered to the processing vessel from the hydrogen fluoride source, preparation comprises Neutral ammonium fluoride (NH 4F) treatment soln; And
(c) a plurality of electronic component predecessor is contacted with said treatment soln, remove the useless material in the electronic component predecessor.
2. according to the process of claim 1 wherein that said electronic component predecessor is a semiconductor wafer.
3. select from the group of ammonium hydroxide and its damping fluid formation according to the process of claim 1 wherein that said ammonium hydroxide is originated.
4. select from the group of hydrofluoric acid and its damping fluid formation according to the process of claim 1 wherein that said hydrogen fluoride is originated.
5. according to the process of claim 1 wherein that said treatment soln also comprises the additive of selecting from the group that tensio-active agent, complexing agent or inhibiter constitute.
6. handle electronic component predecessor's method with the scavenging solution of fluorinated ammonium for one kind, may further comprise the steps:
(a) provide ammonium hydroxide (NH 4OH) source and hydrogen fluoride (HF) source;
(b) ammonium hydroxide is directly delivered in the processing vessel from the ammonium hydroxide source, and hydrogen fluoride is directly delivered to the processing vessel from the hydrogen fluoride source, preparation comprises Neutral ammonium fluoride (NH 4F) treatment soln, in the treatment soln, the volumetric molar concentration of Neutral ammonium fluoride is about 0.02 to 15, hydrofluoric volumetric molar concentration is about 0.01 to 30; And
(c) a plurality of electronic component predecessor is contacted with said treatment soln, remove the useless material in the electronic component predecessor.
7. according to the method for claim 6, wherein said electronic component predecessor is a semiconductor wafer.
8. according to the method for claim 6, wherein said ammonium hydroxide source is selected from the group of ammonium hydroxide and its damping fluid formation.
9. according to the method for claim 6, wherein said hydrogen fluoride source is selected from the group of hydrofluoric acid and its damping fluid formation.
10. according to the method for claim 6, wherein said treatment soln also comprises the additive of selecting from the group that tensio-active agent, complexing agent or inhibiter constitute.
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